CN106832330A - The technique of recovery and the purification of residual lignin after a kind of steam blasting pretreatment - Google Patents
The technique of recovery and the purification of residual lignin after a kind of steam blasting pretreatment Download PDFInfo
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Abstract
The invention discloses the technique of recovery and the purification of residual lignin after a kind of pretreatment of steam blasting.Its technological process is：Get the raw materials ready → pre-preg → steam blasting pre-process → pre-process residue → filtering → air-dry → ball milling → enzymolysis → vacuum drying → extracting → concentration → freeze-drying；Pretreatment fluid → acid is heavy → dialysis → centrifugation → freeze-drying → extracting → concentration → freeze-drying.The present invention is greatly simplified and improves traditional lignin purifying technique, the lignin products of purer function admirable can be obtained, for the recycling of industrial lignin and high level conversion provide good precondition.
Description
Technical field
Recovery the present invention relates to industrial lignin purifies field, and wood is remained after being pre-processed more particularly, to a kind of steam blasting
The technique of recovery and the purification of element.
Background technology
Since 20th century, with the fast development of World Economics, the living standard of people is improved constantly, with population
Surge, demand sharp increase of the world to the energy.The energy is to maintain and promote a motive power for national development, so not
The development country increased rapidly by the developed country or economy that are intense industrialization, its demand to the energy is all with day
Increase.In face of a series of energy crisis and its significant impact for causing, the whole world is all sought to alleviate or even is avoided making great efforts
The measure of energy crisis.Therefore, sight has been placed on renewable, the free of contamination new energy with biomass energy as representative by people
In research.It is by comprehensively utilizing agricultural wastes, forestry waste, special as the cellulosic ethanol of second generation bio-ethanol
The lignocellulosic of the non-grain such as the discarded object of energy crop and various containing celluloses is raw material, by integrating the pre- place of advanced chemistry
Science and engineering skill, biological saccharification and fermentation process are combined with waste gas treatment process, realize the large-scale production of cellulosic ethanol.
Traditional preprocess method is roughly divided into Physical, chemical method, physical-chemical method and bioanalysis.These pretreatments
Technique is intended to by either physically or chemically removing hemicellulose or lignin in wooden structures, so as to effectively improve cellulose
Hydrolysis result.Therefore, substantial amounts of lignin is there is in pretreated waste liquid and in enzymolysis residue, these lignins of good performance
With economic worth very high.For at present, industrial lignin is widely used to petrochemical industry, macromolecular material, industrial diminishing
The field such as agent and medicine synthesis.
The content of the invention
It is an object of the invention to provide the technique of recovery and the purification of residual lignin after a kind of pretreatment of steam blasting.This hair
It is bright to greatly simplify and improve traditional lignin purifying technique, the lignin products of purer function admirable can be obtained, it is industry
The recycling of lignin and high level conversion provide good precondition.
The purpose of the present invention is achieved through the following technical solutions.
The technique of recovery and the purification of residual lignin, comprises the following steps after a kind of steam blasting pretreatment：
(1) get the raw materials ready：By raw material segment, air-dry；
(2) pre-preg：Raw material after step (1) is air-dried is put into the wide-mouth bottle with stirring, adds acid or alkali preimpregnation
Stain, obtains pre-preg liquid；
(3) steam blasting pretreatment：Steamed during step (2) gained pre-preg liquid is added into Moveable steam demolition set
The broken pretreatment of steam explosion, obtains Pretreatment Mixed Liauid；
(4) filter：Pour step (3) gained Pretreatment Mixed Liauid into Buchner funnel suction filtration, must pre-process residue and in advance
Treatment fluid；
(5) air-dry：Pretreatment residue is placed in and dries ventilation and air-dry, until mass dryness fraction is more than 90%；
(6) grind：Residue after step (5) is air-dried grinds in adding planetary ball mill；
(7) digest：Step (6) is ground into gained powder and is placed in enzymolysis in air table；
(8) it is vacuum dried：By step (7) gained enzymolysis liquid vacuum drying；
(9) acid is heavy：Regulation pH=2-5 acid is heavy in putting step (4) gained pretreatment fluid into be loaded with pH meter beaker；
(10) dialyse：Dialysed in putting the heavy gained precipitation of acid into bag filter；
(11) centrifugation：Put the mixture after dialysis into refrigerated centrifuge centrifugation；
(12) freeze-drying：Drying in freeze drier is deposited in after by centrifugation；
(13) extract：Enzymolysis lignin after step (8) is vacuum dried and the lignin after step (12) freeze-drying are carried out
Soxhlet type, concentrated under reduced pressure, freeze-drying, obtain pure lignin.
Preferably, raw material described in step (1) is the former agriculture waste biomass such as maize straw, bagasse, rice straw, straw
Material.
Preferably, the specification of raw material described in step (1) is 5cm × 0.5cm.
Preferably, acid is sulfuric acid described in step (2), and the condition of acid pre-preg is：Solid-liquid ratio is 1:2-1:3, it is sour
Concentration is 3-8wt%, and temperature is room temperature, and the time is 5-15min, and speed of agitator is 150-250r/min；The alkali is ammoniacal liquor, alkali
Property pre-preg condition is：Solid-liquid ratio is 1:3-1:6, the concentration of alkali is 5-30vol%, and temperature is normal temperature, and the time is 6-12h, is stirred
Mix rotating speed is 150-250r/min.
Preferably, the condition of the pretreatment of steam blasting described in step (3) is：Solid-liquid ratio is 1:2-1:6, reaction temperature is
160-180 DEG C, carrying pressure is 0.4-1.0Mpa, and the reaction time is 5-20min.
Preferably, filter paper specification is described in step (4)：Model 102, middling speed.
Preferably, the condition of grinding is described in step (6)：Solid bearing capacity is 10-30g, and temperature is normal temperature, and rotating speed is
450-600rpm, single cycle milling time is 10-20min, and time slot is 10-20min, and cycle-index is 100-150 times.
Preferably, the condition of enzymolysis is described in step (7)：Solid content is 2%, and cellulase bearing capacity is 40-
60FPU/g over dry raw materials, cellobiase bearing capacity is 80-120CBU/g over dry raw materials, and pH is 4.5-5.5, and rotating speed is 150-
300rpm, reaction temperature is 45-55 DEG C, and the reaction time is 48-72h.
Preferably, cellulase described in step (7) is Celluclast 1.5L；The cellobiase is
Novozyme 188；Cushioning liquid used is the citrate buffer solution of 50mmol/L.
Preferably, vacuum drying condition is described in step (8)：It is 35-40 DEG C to set temperature, and drying time is 24-
36h。
Preferably, acid catalysis steam blasting pretreatment fluid 6mol/L NaOH solutions adjust molten during step (9) acid is heavy
Liquid is to pH=2；The base catalysis steam blasting pretreatment fluid H of 3mol/L2SO4Adjust solution to pH=5.
Preferably, the condition of dialysis is described in step (10)：It is 2-3 times/day to change water frequency, and dialysis time is 3-5 days,
The specification of bag filter is 7000-12000Da.
Preferably, the condition of centrifugation is described in step (11)：Centrifugal force is 2000-3000g, and centrifuging temperature is 20 DEG C,
Centrifugation time is 8-12min.
Preferably, the condition of freeze-drying is described in step (12)：Drying temperature：- 50 DEG C, drying time：48-72h.
Preferably, the condition of soxhlet type is described in step (13)：Organic solvent is that volume ratio is 9:1-9.5:The third of 1
Ketone/water, solid-liquid ratio is 1:25-1:35, extraction times are 4-6h；The condition concentrated under reduced pressure is：Thickening temperature is 40-50
DEG C, rotating speed is 15-20rpm；The condition of the freeze-drying is：Drying temperature is -50 DEG C, and drying time is 48-72h.
Compared with prior art, the present invention has the following technical effect that：
The present invention is greatly simplified and improves traditional lignin purifying technique, can obtain the lignin of purer function admirable
Product, for the recycling of industrial lignin and high level conversion provide good precondition.
Brief description of the drawings
Fig. 1 is that dilute sulfuric acid catalytic steam explosion pretreatment fluid reclaims lignin (L1) scanning electron microscope image.
Fig. 2 is dilute sulfuric acid catalytic steam explosion pretreatment residue lignin (L2) scanning electron microscope image.
Fig. 3 is that ammonia-catalyzed steam blasting pretreatment fluid reclaims lignin (L4) scanning electron microscope image.
Fig. 4 is ammonia-catalyzed steam blasting pretreatment residue lignin (L5) scanning electron microscope image.
Specific embodiment
Specific implementation of the invention is further described below in conjunction with accompanying drawing and example, but embodiments of the present invention
Not limited to this.
Embodiment 1
(1) get the raw materials ready：By 300g maize straw segments, air-dry；Maize straw used comes from Northeast China, its main component group
Turn into：28wt% celluloses, 23.6wt% hemicelluloses, 26.6wt% lignins, 4.3wt% ash contents and 4.1wt% benzene alcohol are extracted out
Thing.
(2) pre-preg：Maize straw after step (1) is air-dried is put into the wide-mouth bottle with stirring, and adding concentration is
The sulfuric acid pre-preg of 5% (w/w), obtains pre-preg liquid；The condition of pre-preg is：Solid-liquid ratio (w/w, similarly hereinafter)：1:2.5, temperature：Room
Temperature, time：10min, speed of agitator：150r/min.
(3) steam blasting pretreatment：Step (2) gained pre-preg liquid is added into Moveable steam demolition set (BL-08
Type) in carry out steam blasting pretreatment, obtain Pretreatment Mixed Liauid；Steam blasting pretreatment condition be：Reaction pressure 1.0MPa；
180 DEG C of reaction temperature；Reaction time 15min；Solid-liquid ratio 1:2.5.
(4) filter：Pour step (3) gained Pretreatment Mixed Liauid into Buchner funnel suction filtration, must pre-process residue and in advance
Treatment fluid；Filter paper specification is：Model 102, middling speed.
(5) air-dry：Pretreatment residue is placed in and dries ventilation and air-dry, until mass dryness fraction is more than 90%；
(6) grind：Residue after step (5) is air-dried adds grinding in planetary ball mill (PQ-N2 types)；The bar of grinding
Part is：Solid bearing capacity：10g, temperature：Normal temperature, rotating speed：580rpm, single cycle milling time：10min, time slot：
10min, cycle-index：100 times.
(7) digest：Step (6) is ground into gained powder and is placed in enzymolysis in air table (ZWYR-200D types)；The bar of enzymolysis
Part is：Solid content：2%, cellulase bearing capacity：60FPU/g over dry abrasive flours, cellobiase bearing capacity：120CBU/g
Over dry abrasive flour, pH：4.8, rotating speed：300rpm, reaction temperature：50 DEG C, reaction time：72h.
(8) it is vacuum dried：Step (7) gained enzymolysis liquid is placed in 40 DEG C of vacuum drying 24h in vacuum drying chamber.
(9) acid is heavy：Adjusted with 6mol/L NaOH solutions in putting step (4) gained pretreatment fluid into be loaded with pH meter beaker
Section pH value of solution=2.
(10) dialyse：Dialysed 3 days in putting the heavy gained precipitation of acid into bag filter, change water frequency：2 times/day.
(11) centrifugation：Put the mixture after dialysis into refrigerated centrifuge (H2050R types) centrifugation；Centrifugation
Condition be：Centrifugal force：3000g, operation temperature：20 DEG C, centrifugation time：10min.
(12) freeze-drying：- 50 DEG C of dryings in freeze drier (FD5-series types) are deposited in after by centrifugation
48h；
(13) extract：Enzymolysis lignin after step (8) is vacuum dried and the lignin after step (12) freeze-drying are carried out
Soxhlet type, concentrated under reduced pressure, freeze-drying, obtain lignin sample；The condition of soxhlet type is：Organic solvent：Acetone/water (volume
Than 9:1), solid-liquid ratio：1:30, extraction times：4h；Temperature concentrated under reduced pressure：45 DEG C, rotating speed：15rpm；The condition of freeze-drying
For：Drying temperature：- 50 DEG C, drying time：48h.
The saccharic composition of lignin sample of the present embodiment using chromatography of ions (Dionex ICS-5000) to obtaining is divided
Analysis.IC testing conditions are：Detector：Dionex IonPacTMAG11-HC, chromatographic column：Dionex CarboPac PA20, stream
Dynamic phase：2mmol/L NaOH, flow velocity：0.5mL/min, eluent：200mmol/L NaOH and 1mol/L NaAC.Its detection knot
Fruit is as shown in table 1.
Table 1
L in table 11For sulfuric acid catalysis steam blasting pretreatment fluid reclaims lignin, L2It is pretreatment residue lignin, L3Be without
The raw material milled wood lignin of pretreatment.
As shown in Table 1, by residue lignin L resulting after dilute sulfuric acid catalytic steam explosion pretreatment2Locate with without pre-
Lignin L obtained by the stalk of reason3Compare, with less monose and acid soluble lignin.This is primarily due to preprocessing process and takes off
Except most hemicellulose and the connection between lignin and carbohydrate is broken.And, steam blasting pretreatment promotees
The enzyme hydrolysis process of residue is entered, more celluloses is degraded removing, the enzymolysis lignin higher so as to obtain purity.This
Outward, pretreatment fluid reclaims lignin L1With less ash content, this explanation dialysis procedure is to the inorganic salts tool in removal pretreatment fluid
There is good effect.
The embodiment of the present invention 1 is using Bruker AVANCE III HD 600MHz NMRs to the lignin sample that obtains
The structure of product is analyzed.The 2D-HSQC detections of lignin sample are that 30mg samples are dissolved in the DMSO-d6 of 600 μ L.Operation bar
Part is：Pulse angle is 90 degree, and the time that obtains is 0.11 second, and pulse daley is 1.5 seconds,1JC-HIt is 145,256 scanning.Its inspection
Survey result as shown in table 2.
Table 2
As shown in table 2, most guaiacyl construction units (G) is contained in the lignin of maize straw, next to that lilac
Based structures unit (S), p-hydroxybenzene construction unit (H) is minimum.Secondly, the value of pretreated lignin S/G is significantly improved, this
Because the guaiacyl construction unit of lignin is easiest to removing in diluted acid catalytic steam explosion preprocessing process.This phenomenon master
Containing substantial amounts of 4- vinyl guaiacols (C in pretreatment fluid obtained by being embodied in9H10O2) and vanillic aldehyde (C8H8O3)。
Further, since condensation reaction of the lignin under acidic catalyst, making the side chain area of lignin after pretreatment has little fracture.
The embodiment of the present invention 1 is divided the exterior appearance of gained lignin sample using MERLIN field emission scanning electron microscopes
Analysis.Its scanning electron microscopic picture is as shown in Figure 1 and Figure 2.
As shown in Figure 1 and Figure 2, the pretreated lignin of sulfuric acid catalysis steam blasting shows the surface topography for collapsing, its master
Will be due to the generation of the lignin condensation reaction under the excessive degradation and sulfuric acid catalysis of lignin in preprocessing process.
Embodiment 2
(1) get the raw materials ready：By 300g maize straw segments, air-dry；Maize straw used comes from Northeast China, its main component group
Turn into：28wt% celluloses, 23.6wt% hemicelluloses, 26.6wt% lignins, 4.3wt% ash contents and 4.1wt% benzene alcohol are extracted out
Thing.
(2) pre-preg：Maize straw after step (1) is air-dried is put into the wide-mouth bottle with stirring, and adding concentration is
The ammoniacal liquor pre-preg of 30vol%, obtains pre-preg liquid；The condition of pre-preg is：Solid-liquid ratio (w/w, similarly hereinafter)：1:5, temperature：Room temperature,
Time：6h, speed of agitator：150r/min.
(3) steam blasting pretreatment：Step (2) gained pre-preg liquid is added into Moveable steam demolition set (BL-08
Type) in carry out steam blasting pretreatment, obtain Pretreatment Mixed Liauid；Steam blasting pretreatment condition be：Reaction pressure 0.6MPa；
180 DEG C of reaction temperature；Reaction time 20min；Solid-liquid ratio 1:5.
(4) filter：Pour step (3) gained Pretreatment Mixed Liauid into Buchner funnel suction filtration, must pre-process residue and in advance
Treatment fluid；Filter paper specification is：Model 102, middling speed.
(5) air-dry：Pretreatment residue is placed in and dries ventilation and air-dry, until mass dryness fraction is more than 90%；
(6) grind：Residue after step (5) is air-dried adds grinding in planetary ball mill (PQ-N2 types)；The bar of grinding
Part is：Solid bearing capacity：10g, temperature：Normal temperature, rotating speed：580rpm, single cycle milling time：10min, time slot：
10min, cycle-index：100 times.
(7) digest：Step (6) is ground into gained powder and is placed in enzymolysis in air table (ZWYR-200D types)；The bar of enzymolysis
Part is：Solid content：2%, cellulase bearing capacity：60FPU/g over dry abrasive flours, cellobiase bearing capacity：120CBU/g
Over dry abrasive flour, pH：4.8, rotating speed：300rpm, reaction temperature：50 DEG C, reaction time：72h.
(8) it is vacuum dried：Step (7) gained enzymolysis liquid is placed in 40 DEG C of vacuum drying 24h in vacuum drying chamber.
(9) acid is heavy：Step (4) gained pretreatment fluid is put into the beaker for be loaded with pH meter with the H that concentration is 3mol/L2SO4
Adjust the pH=5 of solution.
(10) dialyse：Dialysed 3 days in putting the heavy gained precipitation of acid into bag filter, change water frequency：2 times/day.
(11) centrifugation：Put the mixture after dialysis into refrigerated centrifuge (H2050R types) centrifugation；Centrifugation
's
Condition is：Centrifugal force：3000g, operation temperature：20 DEG C, centrifugation time：10min.
(12) freeze-drying：- 50 DEG C of dryings in freeze drier (FD5-series types) are deposited in after by centrifugation
48h；
(13) extract：Enzymolysis lignin after step (8) is vacuum dried and the lignin after step (12) freeze-drying are carried out
Soxhlet type, concentrated under reduced pressure, freeze-drying, obtain lignin sample；The condition of soxhlet type is：Organic solvent：Acetone/water (volume
Than 9:1), solid-liquid ratio：1:30, extraction times：4h；Temperature concentrated under reduced pressure：45 DEG C, rotating speed：15rpm；The condition of freeze-drying
For：Drying temperature：- 50 DEG C, drying time：48h.
The saccharic composition of lignin sample of the present embodiment using chromatography of ions (Dionex ICS-5000) to obtaining is divided
Analysis.IC test conditions are with embodiment 1.Its testing result is as shown in table 3.
Table 3
L in table 34For ammonia-catalyzed steam blasting pretreatment fluid reclaims lignin, L5It is pretreatment residue lignin.
As shown in table 3, with L5Compared to L4Containing more carbohydrate, this is pre-processed mainly due to ammonia-catalyzed steam blasting
Maize straw afterwards has enzymolysis property well, and this causes that the most glucans in the maize straw after ball milling are taken off
Remove.Additionally, L4With L1Equally contain little ash content, confirm utilization dialysis process of the present invention except ash content is feasible.
The knot of lignin sample of the present embodiment using Bruker AVANCE III HD 600MHz NMRs to obtaining
Structure is analyzed.2D-HSQC test conditions are with embodiment 1.Its testing result is as shown in table 4.
Table 4
As shown in table 4, the guaiacyl construction unit of lignin is largely removed in preprocessing process so that S/G values increase.
In addition, L4And L5β-the O-4 ' in side chain area, β -5 ', β-β ' and 5-5 ' connection are substantially reduced, and illustrate that ammonia-catalyzed steam blasting is located in advance
Reason has mainly resulted in a large amount of fractures of lignin β-O-4 ' structures and lignin side chain connecting key.This locates in advance with catalysis with acid steam blasting
Reason is very different, and for the latter, the side chain area of lignin is seldom broken.
The present embodiment is analyzed using MERLIN field emission scanning electron microscopes to the exterior appearance of gained lignin sample.It is swept
Retouch electron microscopic picture as shown in Figure 3, Figure 4.
As shown in Figure 3, Figure 4, the lignin for being obtained after the pretreatment of ammonia-catalyzed steam blasting is presented the spherical structure of rule.This
Be probably because alkali lignin there is more preferable dissolubility, can in acetone/water microemulsion system formation rule exterior appearance.Cause
This, compared with acid system lignin, alkali lignin is particularly suited for producing lignin base functional material and Nano microsphere, the preparation of microcapsules.
It is above desirable embodiment of the invention, those skilled in the art completely can be without departing from this invention technological thought
In the range of, carry out various modifications and optimization.And these all of modifications and optimization are included in such as the claims in the present invention institute
Within the scope of restriction, without departing from the Spirit Essence for being included of the invention and required practical scope.
Claims (10)
1. the technique of recovery and the purification of residual lignin after a kind of steam blasting is pre-processed, it is characterised in that comprise the following steps：
（1）Get the raw materials ready：By raw material segment, air-dry；
（2）Pre-preg：To step（1）Acid or alkali pre-preg are added in raw material after air-drying, pre-preg liquid is obtained；
（3）Steam blasting is pre-processed：By step（2）It is quick-fried steam to be carried out in gained pre-preg liquid addition Moveable steam demolition set
Broken pretreatment, obtains Pretreatment Mixed Liauid；
（4）Filtering：By step（3）Gained Pretreatment Mixed Liauid suction filtration, must pre-process residue and pretreatment fluid；
（5）Air-dry：Pretreatment residue is placed in and dries ventilation and air-dry, until mass dryness fraction is more than 90%；
（6）Grinding：By step（5）Residue grinding after air-drying；
（7）Enzymolysis：By step（6）Grinding gained powder is placed in air table and digests；
（8）Vacuum drying：By step（7）Gained enzymolysis liquid is vacuum dried；
（9）Acid is heavy：By step（4）It is heavy that gained pretreatment fluid puts regulation pH=2-5 acid in being loaded with the beaker of pH meters into；
（10）Dialysis：By the heavy gained precipitation dialysis of acid；
（11）Centrifugation：By the mixture centrifugation after dialysis；
（12）Freeze-drying：By the precipitation drying after centrifugation；
（13）Extracting：By step（8）Enzymolysis lignin and step after vacuum drying（12）Lignin after freeze-drying carries out Soxhlet
Extracting, concentrated under reduced pressure, freeze-drying, obtain lignin.
2. technique according to claim 1, it is characterised in that：Step（2）Described in acid be sulfuric acid, the bar of acid pre-preg
Part is：Solid-liquid ratio is 1:2-1:3, the concentration of acid is 3-8wt%, and temperature is room temperature, and the time is 5-15 min, and speed of agitator is
150-250 r/min；The alkali is ammoniacal liquor, and alkaline pre-preg condition is：Solid-liquid ratio is 1:3-1:6, the concentration of alkali is 5-30
Vol%, temperature is normal temperature, and the time is 6-12 h, and speed of agitator is 150-250 r/min.
3. technique according to claim 1, it is characterised in that：Step（3）Described in steam blasting pretreatment condition be：
Solid-liquid ratio is 1:2-1:6, reaction temperature is 160-180 DEG C, and carrying pressure is 0.4-1.0 Mpa, and the reaction time is 5-20
min。
4. technique according to claim 1, it is characterised in that：Step（6）Described in grind condition be：Solid bearing capacity
It is 10-30 g, temperature is normal temperature, and rotating speed is 450-600 rpm, and single cycle milling time is 10-20 min, time slot
It is 10-20 min, cycle-index is 100-150 times.
5. technique according to claim 1, it is characterised in that：Step（7）Described in digest condition be：Solid content is 2-
4%, cellulase bearing capacity is 40-60 FPU/g, and cellobiase bearing capacity is 4.5-5.5 for 80-120 CBU/g, pH, is turned
Speed is 150-300 rpm, and reaction temperature is 45-55 DEG C, and the reaction time is 48-72 h.
6. technique according to claim 1, it is characterised in that：Step（7）Described in cellulase be Celluclast
1.5 L；The cellobiase is Novozyme 188；Cushioning liquid used is the citrate buffer solution of 50 mmol/L.
7. technique according to claim 1, it is characterised in that：Step（8）Described in vacuum drying condition be：Temperature is set
It is 35-40 DEG C to spend, and drying time is 24-36 h.
8. technique according to claim 1, it is characterised in that：Step（10）Described in dialyse condition be：Change water frequency
It it is 2-3 times/day, dialysis time is 3-5 days, the specification of bag filter is 7000-12000 Da.
9. technique according to claim 1, it is characterised in that：Step（11）Described in be centrifuged condition be：Centrifugal force is
2000-3000 g, centrifuging temperature is 20 DEG C, and centrifugation time is 8-12 min.
10. technique according to claim 1, it is characterised in that：Step（13）Described in the condition of soxhlet type be：It is organic
Solvent is that volume ratio is 9:1-9.5:1 acetone/water, solid-liquid ratio is 1:25-1:35, extraction times are 4-6 h；The decompression is dense
The condition of contracting is：Thickening temperature is 40-50 DEG C, and rotating speed is 15-20rpm；The condition of the freeze-drying is：Drying temperature for-
50 DEG C, drying time is 48-72 h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112011066A (en) * | 2019-05-29 | 2020-12-01 | 三通生物工程（潍坊）有限公司 | Production process of high-purity humic acid |
| CN113174770A (en) * | 2021-04-27 | 2021-07-27 | 中南林业科技大学 | Method for pretreating poplar fibers by penetrant synergistic phosphoric acid infiltration coupling steam explosion |
| CN117719039A (en) * | 2024-02-01 | 2024-03-19 | 山东埃尔派粉体科技股份有限公司 | Efficient combined pretreatment method for wood and bamboo |
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| CN113174770A (en) * | 2021-04-27 | 2021-07-27 | 中南林业科技大学 | Method for pretreating poplar fibers by penetrant synergistic phosphoric acid infiltration coupling steam explosion |
| CN117719039A (en) * | 2024-02-01 | 2024-03-19 | 山东埃尔派粉体科技股份有限公司 | Efficient combined pretreatment method for wood and bamboo |
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| CN106832330B (en) | 2020-09-22 |
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